Structures for battery analysis and X-ray diffraction apparatuses

Abstract

The structure for battery analysis of the present invention is equipped with: a pressurizing unit (30) having a pressurizing mechanism, and a pressure receiving unit (10) that receives the pressure acting on the specimen battery (S). The specimen battery (S) accommodated in the hollow portion of the battery accommodating unit (20) is pressurized between the pressurizing unit (30) and the pressure receiving unit (10) to suppress its expansion and contraction.

Description

Technical Field

[0001] The present invention relates to a battery analysis structure used for evaluating all-solid-state batteries by X-ray diffraction measurement, and an X-ray diffraction apparatus equipped with the battery analysis structure. Background Art

[0002] An all-solid-state battery has a structure in which electrode active material layers are provided on both end sides of an electrolyte layer, and capacity deterioration and resistance increase occur during charge and discharge cycles. For example, in an all-solid-state lithium ion battery, since changes in crystal structure are likely to occur along with the insertion and extraction of lithium ions (Li), in order to clarify the deterioration mechanism, the changes in crystal structure accompanying charge and discharge are evaluated by X-ray diffraction measurement. Patent Documents 1 and 2 disclose conventional battery analysis structures for evaluating a test battery by X-ray diffraction measurement.

[0003] The X-ray measurement battery structure disclosed in Patent Document 1 has the following structure: a battery element (2) is sandwiched between a negative electrode side cover (5a) and a positive electrode side cover (5b), and each cover (5a, 5b) is fastened with a plurality of nuts (22) to seal the battery element (2) and isolate the battery element (2) from the atmosphere. In addition, the fastening structure formed by the nuts (22) is used to ensure the airtightness of the battery element (2) (refer to paragraph

[0020] of the specification of this Document 1).

[0004] In addition, the analysis unit disclosed in Patent Document 2 has a housing (10) including a first component (11), a second component (21), and a third component (31). A test battery (100) is accommodated in the housing (10), and evaluation is performed by X-ray diffraction measurement. For each component (11, 21, 31) constituting the housing (10), the components are assembled by inserting bolts into a plurality of through holes (12, 22, 32) provided in the respective components and tightening with nuts. (Refer to paragraph

[0053] of the specification of this Document 2).

[0005] In addition, in each patent document, symbols in parentheses are assigned to each component (the same applies hereinafter).

[0006] In an all-solid-state battery, a solid electrolyte is used for the electrolyte layer. Inside the all-solid-state battery, elements such as the electrode active material layer, the solid electrolyte layer, and the conductive material expand and contract during charge and discharge, and phenomena such as voids between particles, peeling at the interface between the solid electrolyte layer and the electrode active material layer, or internal cracks are likely to occur. In the case where these phenomena occur, the battery cannot function properly. Therefore, when analyzing and evaluating such an all-solid-state battery as a test battery, it is necessary to hold the test battery in a pressurized state, ensure the conduction path, and suppress the expansion and contraction accompanying charge and discharge.

[0007] However, none of the conventional battery analysis structures (analysis units) disclosed in the above-mentioned Patent Documents 1 and 2 have a structure for holding the test battery in a pressurized state to ensure a conduction path or suppress the expansion and contraction of the test battery during charge and discharge.

[0008] Incidentally, the fastening structure formed by the nut (22) disclosed in Patent Document 1 is for ensuring the airtightness of the battery element (2). Moreover, since elastic members (4a, 4b) are interposed therebetween, even if the nut (22) is tightened, it is impossible to apply a large pressure to the test battery to such an extent that a conduction path can be ensured or expansion and contraction can be suppressed.

[0009] In addition, a pressing mechanism (46) composed of a push rod is disclosed in Patent Document 2, and this pressing mechanism (46) is for causing a part of the electrode active material (112), the test electrode (110), and the window member (51), which are elements of the test battery, to protrude from the window portion (13) of the frame (10) (refer to paragraph

[0042] of the specification of this Document 2 and Figure 3 ).

[0010] In this way, by causing a part of the electrode active material (112), the test electrode (110), and the window member (51) to protrude from the window portion (13) of the frame (10), the window member (51) is used to cover the surroundings of the electrode active material (112) and the test electrode (110) to prevent the electrolyte from invading between the test electrode (110) and the window member (51), thereby improving the airtightness of the test electrode (refer to paragraph

[0054] of the specification of this Document 2).

[0011] However, in the pressing mechanism (46) of this Document 2, since there is no component on the side opposite to the push rod to withstand the pushing force of the push rod, it is a structure in which the window member (51) is both stretched and subjected to this pushing force. Therefore, even with this pressing mechanism (46), it is impossible to apply a large pressure to the test battery to such an extent that a conduction path can be ensured or expansion and contraction can be suppressed.

[0012] In addition, since each element constituting the all-solid-state battery is a material that reacts with moisture or air, the operation of accommodating the battery and assembling the battery analysis structure (analysis unit) needs to be carried out in an environment where each element of the test battery does not come into contact with moisture or air. For example, in the case of using an all-solid-state lithium-ion battery as the test battery, the assembly operation of this structure is carried out inside a glove box in which the internal space is in a high-purity argon atmosphere. The operator performs the assembly operation of this structure by operating from the outside through the gloves.

[0013] However, in the prior art disclosed in the above patent documents, since the operation of tightening a plurality of nuts is required during assembly, there is a drawback that the assembly operation in the glove box becomes complicated.

[0014] Prior art documents

[0015] Patent documents

[0016] Patent Document 1: Japanese Patent Application Laid-Open No. 2012-159311

[0017] Patent Document 2: Japanese Patent Application Laid-Open No. 2017-72530 Summary of the Invention

[0018] Problems to be Solved by the Invention

[0019] The present invention has been completed in view of the above circumstances. The first object of the present invention is to provide a battery analysis structure capable of pressurizing a specimen battery to suppress its expansion and contraction.

[0020] In addition, the second object of the present invention is to provide a battery analysis structure capable of accommodating and sealing a specimen battery with a simple assembly operation and realizing the analysis and evaluation of a specimen battery for X-ray diffraction measurement in the atmosphere.

[0021] Furthermore, the third object of the present invention is to provide an X-ray diffraction apparatus capable of accurately measuring a specimen battery using such a battery analysis structure.

[0022] Means for Solving the Problems

[0023] The battery analysis structure of the present invention is provided with: a battery accommodation unit having a hollow portion for accommodating a specimen battery; a pressurizing unit mounted on one end face side of the battery accommodation unit and equipped with a pressurizing mechanism for applying pressure to the specimen battery accommodated in the hollow portion of the battery accommodation unit; and a pressure receiving unit fixed to the other end face side of the battery accommodation unit to receive the pressure acting on the specimen battery. In the pressure receiving unit, an X-ray window is formed by a cutout hole penetrating from the front surface to the back surface, and the X-ray window is used to irradiate the specimen battery accommodated in the hollow portion of the battery accommodation unit with X-rays and to emit the diffracted X-rays reflected from the specimen battery to the outside. In the X-ray window, a partition member is disposed, and the partition member allows X-rays to pass through but isolates the hollow portion in the battery accommodation unit from the atmosphere.

[0024] The present invention configured in this way can pressurize the specimen battery accommodated in the hollow portion of the battery accommodation unit between the pressurizing unit and the pressure receiving unit to ensure its conduction path or suppress expansion and contraction.

[0025] In addition, the pressure receiving unit and the battery accommodating unit may also be integrally formed and constituted by one unit.

[0026] In addition, preferably, the X-ray window is formed with a smaller width compared to the pressing region where the test battery accommodated in the hollow portion of the battery accommodating unit abuts against the partitioning member.

[0027] By forming the X-ray window with such a width, it is possible to ensure a sufficient area on the back surface of the pressure receiving unit to withstand the pressure from the pressurizing unit.

[0028] In addition, the pressurizing mechanism may be formed in such a structure that it at least has a bolt member for adjusting the pressure applied to the test battery, and a nut portion that is threadedly engaged with the bolt member is formed in the pressurizing unit. Further, a structure may be formed such that a pressing member is inserted into the hollow portion of the battery accommodating unit, and the test battery receives the pressure from the bolt member via the pressing member.

[0029] With this structure, a desired pressure can be applied to the test battery by a simple operation of screwing in one bolt member.

[0030] In particular, since all-solid-state batteries are prone to generating voids between particles caused by expansion and contraction during repeated charge and discharge, peeling at the interface between the solid electrolyte layer and the electrode active material layer, or internal cracks, etc., and cannot function properly as a battery, a high pressure needs to be applied at all times during experiments. In order to smoothly carry out appropriate evaluation operations, preferably, a structure capable of pressurizing the test battery through a simple operation is provided to form such a pressurized state.

[0031] In addition, the present invention may be formed with a structure equipped with an insulating member that is embedded in the hollow portion of the battery accommodating unit to insulate the outer peripheral surface of the test battery accommodated in the hollow portion and to close the X-ray window. The front end surface of the insulating member is pressed against the partitioning member via an airtight member, and the partitioning member is in close contact with the periphery of the X-ray window by this pressing force to close the X-ray window.

[0032] With such a structure, it is possible to ensure insulation of the outer peripheral surface of the test battery using the insulating member and to hermetically seal the X-ray window.

[0033] In addition, the present invention may also be formed with a structure in which internal and external thread portions are provided between one end surface side of the battery accommodating unit and one end surface side of the pressurizing unit mounted on the one end surface side, and the one end surface side of the pressurizing unit is mounted on the one end surface side of the battery accommodating unit by screwing in operation of the thread portions to seal between the units.

[0034] With such a structure, the pressurizing unit can be installed in the battery housing unit by a simple operation of screwing in the pair of inner and outer threaded portions, and the hollow portion in the battery housing unit that houses the test battery can be sealed.

[0035] Thus, even when the assembly operation is carried out from the outside of the glove box through gloves, the operator can easily perform this operation. In addition, even when the assembly operation is carried out in a relatively large space such as a drying chamber, the operation is equally easy.

[0036] In addition, a structure can be formed such that for the pressurizing unit, the pressurizing mechanism is exposed on the other end face side where no threaded portion is provided, and the pressurizing operation is carried out from this other end face side. In such a configuration, it is preferable to form a structure equipped with an airtight housing unit that airtightly seals the periphery of the pressurizing mechanism exposed on the other end face side of the pressurizing unit, and inner and outer second threaded portions are provided between the other end face side of the pressurizing unit and one end face side of the airtight housing unit installed on this other end face side. By screwing in operation of these second threaded portions, one end face side of the airtight housing unit is installed on the other end face side of the pressurizing unit and sealed.

[0037] By configuring in this way, the space on the other end face side of the pressurizing unit where the pressurizing mechanism is exposed can be made airtight by the airtight housing unit.

[0038] The test battery is formed, for example, in such a structure that electrode active material layers are arranged on both end sides of the electrolyte layer, and further, current collector layers are respectively arranged outside each electrode active material layer.

[0039] When such a configured test battery is taken as an analysis object, it is preferable to form a structure having a first electrode terminal and a second electrode terminal provided on the outside, the first electrode terminal being electrically connected to one current collector layer, and the second electrode terminal being electrically connected to the other current collector layer.

[0040] By connecting between these respective electrode terminals and a charge and discharge device, the test battery can be charged and discharged, and the evaluation of the test battery during the charge and discharge cycle can be continuously carried out.

[0041] Here, a structure can be formed such that the first electrode terminal is provided outside the pressure receiving unit, and the pressure receiving unit is composed of a conductive metal component, and one current collector layer is electrically connected to the first electrode terminal via this pressure receiving unit.

[0042] In addition, a structure can be formed such that the pressurizing mechanism is composed of a conductive metal component, and the other current collector layer is electrically connected to the second electrode terminal via this pressurizing mechanism.

[0043] Furthermore, the present invention can form a structure in which the separating member is constituted as one of the current collector layers constituting the test cell, and the pressing mechanism presses the test cell and the separating member against the back surface of the pressure receiving unit so that the separating member is in close contact with one of the electrode active material layers constituting the test cell.

[0044] Thereby, it is not necessary to separately prepare the separating member, and the number of components is reduced by one.

[0045] Here, when pressure acts on the current collector layer disposed at the back opening of the X-ray window, there is a risk that a part of the current collector layer is pressed into the cutout hole forming the X-ray window, resulting in unevenness or wrinkles.

[0046] Therefore, it is preferable to form a structure equipped with a block holder configured to be inserted from the front opening of the X-ray window, and the front end face is buried in the back opening of the X-ray window.

[0047] By burying the front end face of the block holder in the back opening of the X-ray window, it is possible to prevent a part of the current collector layer from being pressed into the X-ray window.

[0048] In addition, a structure can be formed in which the pressing unit is equipped with an output unit that outputs an electrical signal related to the pressure acting on the pressing member. By measuring the pressure acting on the pressing member using the electrical signal output from this output unit, it is possible to measure the volume change of the test cell accompanying charge and discharge using a pressure gauge, and to analyze and evaluate the correlation with the crystal structure change.

[0049] Furthermore, the present invention can form a structure in which a concave portion is provided around the back surface of the X-ray window formed in the pressure receiving unit, and a thin plate-like vitreous carbon (glass carbon) or beryllium is disposed in the concave portion.

[0050] Vitreous carbon or beryllium, which is called glass carbon, has the property of transmitting X-rays and isolating the atmosphere. Moreover, due to its high pressure resistance, even when subjected to the pressure acting on the test cell, it will not be pressed into the cutout hole of the X-ray window, and can support the separating member and the test cell with a flat surface.

[0051] In addition, the present invention can also be formed into a structure equipped with a positioning abutting portion that abuts against the positioning portion provided on the X-ray diffractometer to position the X-ray window with respect to the X-rays irradiated from the X-ray diffractometer.

[0052] Here, if the positioning abutting portions are provided at two positions that are symmetric with respect to the rotation center when rotating freely with respect to the X-ray diffractometer, the X-rays are incident from directions that are 180 degrees different with respect to the X-ray window.

[0053] In addition, the present invention can also be formed into a structure equipped with a base, which is disposed on a mounting table formed by a circular groove provided in an X-ray diffractometer, has a circular bottom surface and a circumferential surface, and is rotatably guided by the circular groove of the mounting table.

[0054] Thus, by providing a base that can be rotatably supported only by being disposed in the circular groove provided in the X-ray diffractometer, the installation operation for the X-ray diffractometer can be facilitated.

[0055] Next, the X-ray diffractometer according to the present invention is characterized in that it has the following structure: a battery analysis structure body as described above is installed, and X-rays are irradiated onto a sample battery accommodated in the hollow portion of the battery accommodation unit through an X-ray window, thereby performing X-ray diffraction measurement.

[0056] Thereby, high-precision X-ray diffraction measurement of the sample battery can be achieved.

[0057] In addition, the X-ray diffractometer according to the present invention can also be formed into a structure having a positioning block and a slit device. The positioning block has a positioning portion for positioning the X-ray window of the battery analysis structure body, and the slit device is detachably attached to the positioning block and is used to reduce X-ray scattering generated from sources other than the sample battery accommodated in the hollow portion of the battery accommodation unit.

[0058] By introducing this slit device, higher-precision X-ray diffraction measurement can be achieved.

[0059] As described above, according to the present invention, the sample battery can be held in a pressurized state, and analysis and evaluation of the sample battery by X-ray diffraction measurement can be achieved while suppressing expansion and contraction accompanying charge and discharge. BRIEF DESCRIPTION OF THE DRAWINGS

[0060] Figure 1 It is a perspective view showing the appearance of a battery analysis structure body according to a first embodiment of the present invention.

[0061] Figure 2 It is a front cross-sectional view showing the overall structure of a battery analysis structure body according to a first embodiment of the present invention.

[0062] Figure 3 It is an exploded perspective view of a battery analysis structure body according to a first embodiment of the present invention.

[0063] Figure 4 It is an exploded front cross-sectional view of a battery analysis structure body according to a first embodiment of the present invention.

[0064] Figure 5It is an exploded perspective view showing the structures of the pressure receiving unit and the battery accommodating unit.

[0065] Figure 6A It is a front cross-sectional view for explaining the arrangement of the current collector layer on the back surface of the pressure receiving unit and the pressing function generated by the insulating member. Figure 6B It is a top view showing the arrangement relationship of the X-ray window, the current collector layer, and the specimen battery. Figure 6C It is a front cross-sectional view for explaining the function of the block holder.

[0066] Figure 7A It is a perspective view for explaining the implementation of X-ray diffraction measurement using the battery analysis structure according to the first embodiment of the present invention. Figure 7B It is a bottom view for explaining the adjustment of the orientation between the reference end surface of the base and the X-ray window.

[0067] Figure 8 It is a flowchart for explaining the analysis and evaluation method of the specimen battery using the battery analysis structure according to the first embodiment of the present invention.

[0068] Figure 9 It is a graph showing the results of observing the state change (phase state change accompanying the insertion and extraction of lithium ions) during the charge and discharge process of the negative electrode active material for all-solid-state batteries using the battery analysis structure according to the first embodiment of the present invention with an X-ray diffraction apparatus.

[0069] Figure 10 It is a perspective view showing the appearance of the battery analysis structure according to the second embodiment of the present invention.

[0070] Figure 11 It is an exploded front cross-sectional view of the battery analysis structure according to the second embodiment of the present invention.

[0071] Figure 12 It is a perspective view showing the mounting table for mounting the battery analysis structure according to the second embodiment of the present invention on an X-ray diffraction apparatus.

[0072] Figure 13 It is a perspective view for explaining the operation of mounting the battery analysis structure on the mounting table.

[0073] Figure 14 It is a perspective view showing the state of arranging the battery analysis structure in the circumferential groove of the mounting table.

[0074] Figure 15 It is a perspective view for explaining the positioning structure provided between the mounting table and the battery analysis structure.

[0075] Figure 16It is a perspective view for explaining a slit device provided on an installation table.

[0076] Figure 17 It is a perspective view showing the appearance of an X-ray diffraction apparatus for analyzing a mounted battery analysis structure.

[0077] Figure 18 It is a front cross-sectional view for explaining a modified example of the present invention.

[0078] Explanation of reference numerals

[0079] S: Specimen battery, 1: Battery analysis structure

[0080] 10: Pressure receiving unit, 11: X-ray window, 12: Partition member (current collector layer), 13: Block holder, 14: Convex portion, 15: First electrode terminal

[0081] 20: Battery accommodation unit, 21: Insulating member, 21a: Flange portion, 22: Pushing member, 23: External thread portion

[0082] 30: Pressurizing unit, 30A: Outer main body portion, 30B: Inner main body portion, 31: Nut portion, 32: Bolt member, 33: Pressure transmission member, 34: Load cell, 34a: Output rod (output portion), 35: Internal thread portion, 36: Metal ring, 37: Second external thread portion

[0083] 40: Hermetic housing unit, 41: Second internal thread portion, 42: Second electrode terminal, 43: Conductive member, 44: Base, 44a: Reference end face, 45: Long hole

[0084] 50: Fastener, 51: O-ring (hermetic member), 52: Operating rod (positioning abutting portion)

[0085] 60: Window embedding member, 61: Recess

[0086] 100: Pressure receiving and battery housing unit, 101: Base portion

[0087] 200: Installation table, 201: Circumferential groove, 202: Positioning block, 202a: Positioning portion, 203: Slit device, 210: Slit device, 210: X-ray source, 220: X-ray detector Detailed description of the embodiments

[0088] Hereinafter, embodiments of the present invention will be described in detail with reference to the drawings.

[0089] The specimen battery to be analyzed and evaluated has a structure in which electrode active material layers are disposed on both end sides of an electrolyte layer, and further, current collector layers are disposed outside each electrode active material layer.

[0090] Conventional batteries such as lithium-ion batteries use electrolytes with a liquid or gel-like electrolyte layer. However, in all-solid-state batteries developed in recent years, a solid electrolyte is used for the electrolyte layer. Inside an all-solid-state battery, due to the expansion and contraction generated during charge and discharge, voids between particles, peeling at the interface between the solid electrolyte layer and the electrode active material layer, or internal cracks are likely to occur. In the case where these phenomena occur, the battery cannot function properly. Therefore, when analyzing and evaluating such an all-solid-state battery as a test battery, it is necessary to maintain the test battery in a pressurized state to ensure the conduction path associated with charge and discharge and suppress expansion and contraction.

[0091] In addition, as already described, each element constituting the all-solid-state battery is a material that reacts with water or air. Therefore, the operation of assembling the battery analysis structure is usually carried out in a space such as inside a glove box (GB) under an atmosphere of high-purity argon gas as an inert gas.

[0092] And, the test battery accommodated inside the battery analysis structure in a sealed state is analyzed and evaluated using an X-ray diffraction device in the atmosphere. Here, for the X-ray diffraction device, it is preferable to use a reflection-type X-ray diffraction device with high versatility for analysis and evaluation.

[0093] The battery analysis structure according to each embodiment of the present invention described below forms a structure that satisfies all of the above conditions.

[0094] 〔First Embodiment〕

[0095] First, with reference to Figures 1 to 9 , the battery analysis structure according to the first embodiment of the present invention will be described in detail.

[0096] Figure 1 is a perspective view showing the appearance of the battery analysis structure according to the present embodiment, Figure 2 is a front cross-sectional view showing the overall structure of the battery analysis structure. Further, Figure 3 is an exploded perspective view of the battery analysis structure according to the present embodiment, Figure 4 is its exploded front cross-sectional view.

[0097] As shown in Figure 3 and Figure 4 , the constituent elements of the battery analysis structure include: a pressure receiving unit 10, a battery accommodation unit 20, a pressurizing unit 30, and an airtight housing unit 40. The pressurizing unit 30 is installed on one end face side (the lower end face side in the figure) of the battery accommodation unit 20, and the pressure receiving unit 10 is installed on the other end face side (the upper end face side in the figure) of the battery accommodation unit 20.

[0098] The sample cell S to be analyzed is housed in the cell housing unit 20 and is isolated from the atmosphere in a sealed state.

[0099] Figure 5 It is an exploded perspective view showing the structures of the pressure receiving unit and the cell housing unit.

[0100] As Figures 3 to 5 shown, the pressure receiving unit 10 is formed in a disc shape, and an X-ray window 11 in a long hole shape extending in the diameter direction along the center is formed by a cut hole penetrating from the front to the back (refer to Figure 5 ). In addition, the shape of the X-ray window 11 is not limited to the long hole shape, and it may be formed into other shapes such as a circle or a rectangle according to needs.

[0101] The pressure receiving unit 10 is press-fitted and fixed to the cell housing unit 20 by a fastener 50 such as a bolt.

[0102] The cell housing unit 20 is formed in a cylindrical shape, and the sample cell S is housed in a hollow portion having a circular cross-section formed therein. To ensure strength, the cell housing unit 20 is preferably made of a metal material. If the cell housing unit 20 is made of a metal material, the sample cell S housed in the hollow portion will be electrically short-circuited. Therefore, a cylindrical insulating member 21 is inserted into the hollow portion of the cell housing unit 20, and the sample cell S is housed in the hollow portion of the insulating member 21. Thus, the outer peripheral surface of the sample cell S is insulated by the insulating member 21. The insulating member 21 is formed of a synthetic resin material having insulating properties.

[0103] For the insulating member 21, preferably, insulating members of various sizes in which the inner diameter of the hollow portion is adapted to the diameters of various sample cells S to be analyzed and evaluated are prepared in advance and used by replacing according to the sample cell S.

[0104] A partition member 12 is disposed on the back side of the X-ray window 11 of the pressure receiving unit 10 to isolate the hollow portion in the cell housing unit 20 from the atmosphere. The partition member 12 is formed of a material that allows X-rays to pass through but does not allow air or moisture to pass through.

[0105] In the present embodiment, one of the current collector layers disposed on both sides of the sample cell S is used as the partition member 12. The current collector layer is composed of a metal foil such as conductive aluminum foil or copper foil, and since this metal foil has the property of allowing X-rays to pass through but not allowing air or moisture to pass through, it is suitable for use as the partition member 12. Therefore, in the present embodiment, one of the current collector layers of the sample cell S is separated, and this current collector layer is disposed on the back of the pressure receiving unit 10 to cover the X-ray window 11.

[0106] In addition, in the present embodiment, the insulating member 21 functions as a pressing mechanism for pressing the separating member 12 (current collector layer) against the back surface of the pressure receiving unit 10.

[0107] That is, as Figure 6A shown, the separating member 12 (current collector layer) is disposed on the back surface of the pressure receiving unit 10, and the insulating member 21 presses the separating member 12 against the back surface of the pressure receiving unit 10 to bring them into close contact. As Figure 6B shown, the separating member 12 (current collector layer) is disposed so as to cover the X-ray window 11 formed in the pressure receiving unit 10, and the insulating member 21 brings the separating member 12 into close contact with the back surface of the pressure receiving unit 10, whereby it is possible to prevent the intrusion of the atmosphere from the X-ray window 11 with high precision.

[0108] In addition, when the separating member 12 is not constituted by the current collector layer, the separating member 12 may be attached to the back surface of the pressure receiving unit 10 to seal the X-ray window 11. In this case, the insulating member 21 may not function as a pressing mechanism.

[0109] In the pressure receiving unit 10, as Figure 6A and Figure 6B shown, the sample cell S is disposed at a position facing the X-ray window 11 with the separating member 12 (current collector layer) interposed therebetween. And, as will be described later, the sample cell S is pressed against the back surface of the pressure receiving unit 10 with an arbitrary pressure.

[0110] The pressure receiving unit 10 has a function of receiving the pressure acting on the sample cell S.

[0111] In addition, as Figure 6A shown, the X-ray window 11 has a function of irradiating the sample cell S disposed on the back surface side of the pressure receiving unit 10 with X-rays, and allowing the diffracted X-rays reflected from the sample cell S to be emitted to the outside.

[0112] Here, as Figure 6B shown, in order to ensure a sufficient area for receiving the pressure from the sample cell S on the back surface of the pressure receiving unit 10, the width of the X-ray window 11 is at least smaller than the width of the sample cell S. In addition, as Figure 6A shown, preferably, the length and the thickness of the inner wall of the X-ray window 11 are determined in consideration of the measurement range (incident angle θ of X-rays and diffraction angle 2θ to be detected) of the X-ray diffraction measurement required by the analyst of the sample cell S or the pressing conditions of the sample cell S, etc.

[0113] On the front end face of the insulating member 21, an O-ring 51 is disposed as an airtight member for pressing the separating member 12 (current collector layer) against the back surface of the pressure receiving unit 10. Further, in Figure 2 , Figure 4 , Figure 6A , Figure 6C , Figure 10 , the hatching of the O-ring 51 is omitted in the sectional view.

[0114] In the insulating member 21, as Figure 5 shown, a flange portion 21a extending in the outer diameter direction from the base end edge is formed, and the flange portion 21a is fastened to one end face side of the battery housing unit 20 by a fastener 50 such as a bolt. By the fastening force (pushing force) at this time, the separating member 12 (current collector layer) is pressed against the back surface of the pressure receiving unit 10 via the O-ring 51 (see Figure 4 ). Thereby, the separating member 12 (current collector layer) is in close contact with the periphery of the X-ray window 11, and the X-ray window 11 is closed.

[0115] Since the operation of installing the pressure receiving unit 10 to the other end face side of the battery housing unit 20 by the fastener 50, the operation of inserting the separating member 12 (current collector layer) into the hollow portion of the pressure receiving unit 10 to be disposed on the back surface of the pressure receiving unit 10, and the operation of embedding the insulating member 21 into the hollow portion of the pressure receiving unit 10 and fastening its flange portion 21a to one end face side of the pressure receiving unit 10 by the fastener 50 are all operations that do not process the main body of the specimen battery S (except for the current collector layer as the separating member 12), they can be performed in the atmosphere. Therefore, the operation of fastening a plurality of bolts or the like of the fastener 50 is not troublesome and can be performed relatively easily.

[0116] As Figures 3 to 5 shown, the battery analysis structure of the present embodiment is provided with a block holder 13. The block holder 13 is mounted on the surface of the pressure receiving unit 10 by a fastener 50 such as a bolt. A convex portion 14 corresponding to the size and shape of the X-ray window 11 is formed on the block holder 13 (see Figure 5 ), and the convex portion 14 is embedded in the X-ray window 11, and its front end face is disposed on the same plane as the back surface opening of the X-ray window 11, and has a function of burying the back surface opening to eliminate a large recess.

[0117] As Figure 6C shown, in the X-ray window 11, the separating member 12 (current collector layer) is disposed from the back surface side, and further, as will be described later, the specimen battery S is pressed. There is a risk that the separating member 12 is pushed into the cutout hole of the X-ray window 11 by the pressure applied to the specimen battery S, resulting in wrinkles or cracks and the breakdown of the airtight state.

[0118] Therefore, the block holder 13 is pre - installed on the pressure - bearing unit 10 to substantially eliminate the recess in the back opening of the X - ray window 11, and the separator 12 (current collector layer) is supported by a substantially flat surface. Thus, problems such as wrinkles or cracks in the separator 12 (current collector layer) can be avoided.

[0119] Return Figures 2 to 4 , and the pressurizing unit 30 has a function of applying pressure to the specimen battery S accommodated in the hollow portion of the battery accommodation unit 20 (specifically, in the hollow portion of the insulating member 21).

[0120] The pressurizing unit 30 has a cylindrical main body. The main body is composed of an outer main body 30A and an inner main body 30B. The same cylindrical inner main body 30B is embedded in the interior (hollow portion) of the cylindrical outer main body 30A and is integrated by fixing with fasteners 50 such as bolts (see Figure 4 ).

[0121] Here, the outer main body 30A is made of a synthetic resin material having electrical insulation properties, strength capable of withstanding the reaction of the applied pressure, and airtightness (for example, polyvinyl chloride (PVC), polyvinylidene chloride (PVdC), polystyrene (PS), acrylonitrile - styrene copolymer (AS resin), acrylonitrile - butadiene - styrene copolymer (ABS resin), high - density polyethylene (HDPE), polypropylene (PP), polyoxymethylene (POM), polymethyl methacrylate (PMMA), methyl methacrylate - styrene copolymer (MS), polycarbonate (PC), polychlorotrifluoroethylene (PCTFE), polytetrafluoroethylene (PTFE), etc.). On the other hand, the inner main body 30B is made of a metal material having strength capable of withstanding the reaction force of the applied pressure.

[0122] As Figure 4 shown, the inner peripheral surface of the inner main body 30B is formed in a stepped shape, and a nut portion 31 is formed on the inner peripheral surface of the rear part with a smaller inner diameter. A bolt member 32 is threadedly engaged with the nut portion 31. The bolt member 32 constitutes a pressurizing mechanism for applying pressure to the specimen battery S accommodated in the hollow portion of the battery accommodation unit 20. In addition, as will be described later, the bolt member 32 forms a conduction path for charging and discharging the specimen battery S. Therefore, it is made of a metal material having strength to apply high pressure to the specimen battery S and having conductivity.

[0123] The pressure transmission member 33 is slidably fitted into the inner circumferential surface of the front portion of the inner side main body portion 30B having a large inner diameter, and the force measuring sensor 34 serving as a pressure measuring mechanism is assembled to the pressure transmission member 33. The force measuring sensor 34 measures the pressure generated by screwing in the bolt member 32, and outputs an electric signal indicating the measured value thereof to a pressure display (not shown in the figure) via the output rod 34a (output portion). By measuring the pressure in this way, the correlation between the pressure acting on the sample cell S and the change in the crystal structure generated during the charge and discharge of the sample cell S can be analyzed and evaluated.

[0124] As will be described later, the pressure transmission member 33 and the force measuring sensor 34 also form a conduction path for charging and discharging the sample cell S. Therefore, they are formed of a conductive metal material.

[0125] In addition, as the pressure measuring mechanism, it is not limited to the force measuring sensor. For example, a torque wrench can be used instead of the force measuring sensor, and the pressure can be obtained from the torque acting on the bolt member 32.

[0126] As Figure 2 shown, the pressurizing unit 30 is mounted on one end face side (the lower end face side in the figure) of the battery housing unit 20. And, a cylindrical pressing member 22 is inserted into the hollow portion of the battery housing unit 20 (specifically, into the hollow portion of the insulating member 21).

[0127] The pressing member 22 is interposed between the force measuring sensor 34 and the sample cell S, and has a function of pressing the sample cell S in the direction of the pressure receiving unit 10 by the pressing force from the bolt member 32. That is, along with the screwing operation of the bolt member 32, the pressing force acts on the sample cell S via the pressure transmission member 33, the force measuring sensor 34, and the pressing member 22, and the sample cell S is pressed against the pressure receiving unit 10.

[0128] Thereby, the sample cell S can be pressurized. For the pressurization value, it can be arbitrarily set by adjusting the screwing amount of the bolt member 32 while referring to the display of the pressure display (not shown).

[0129] Here, as will be described later, the pressing member 22 also forms a conduction path for charging and discharging the sample cell S. Therefore, it is formed of a conductive metal material.

[0130] As Figures 2 to 4As shown, the airtight housing unit 40 is formed in a cylindrical shape, and one end face side (the upper end face side in the figure) is mounted on the other end face side (the lower end face side in the figure) of the pressurizing unit 30. On the other hand, the flat base 44 is fixed to the other end face side (the lower end face side in the figure) of the airtight housing unit 40 by fasteners 50 such as bolts. Therefore, by being mounted on the other end face side of the pressurizing unit 30, the periphery of this other end face side is sealed by the airtight housing unit 40 and isolated from the atmosphere.

[0131] The head of the bolt member 32 provided in the pressurizing unit 30 is exposed on the other end face side of this unit and is disposed within the hollow portion of the airtight housing unit 40. Since a sealed space is formed within the hollow portion of the airtight housing unit 40, it is possible to prevent air from invading into the battery housing unit 20 through the minute gap at the portion where the bolt member 32 engages with the nut portion 31.

[0132] The airtight housing unit 40 is formed of a synthetic resin material having electrical insulation properties (for example, polyvinyl chloride (PVC), polyvinylidene chloride (PVdC), polystyrene (PS), acrylonitrile-styrene copolymer (AS resin), acrylonitrile-butadiene-styrene copolymer (ABS resin), high-density polyethylene (HDPE), polypropylene (PP), polyoxymethylene (POM), polymethyl methacrylate (PMMA), methyl methacrylate-styrene copolymer (MS), polycarbonate (PC), polychlorotrifluoroethylene (PCTFE), polytetrafluoroethylene (PTFE), etc.).

[0133] On one end face side (the lower end face side in the figure) of the battery housing unit 20, an external thread portion 23 is provided. On the other hand, on one end face side (the upper end face side in the figure) of the pressurizing unit 30 mounted on this one end face side, an internal thread portion 35 is provided. And a structure is formed such that by threadedly mating these external thread portion 23 and internal thread portion 35 and performing a screwing operation, the one end face side of the pressurizing unit 30 is mounted on the one end face side of the battery housing unit 20.

[0134] In addition, on the other end face side (the lower end face side in the figure) of the pressurizing unit 30, a second external thread portion 37 is provided. On the other hand, on one end face side (the upper end face side in the figure) of the airtight housing unit 40 mounted on this other end face side, a second internal thread portion 41 is provided. And a structure is formed such that by threadedly mating these second external thread portion 37 and second internal thread portion 41 and performing a screwing operation, the one end face side of the airtight housing unit 40 is mounted on the other end face side of the pressurizing unit 30.

[0135] Thus, through a simple operation of screwing in a pair of inner and outer threaded portions, the pressurizing unit 30 can be installed in the battery housing unit 20, and the space between the battery housing unit 20 containing the test battery S and the pressurizing unit 30 can be sealed. Similarly, through a simple operation of screwing in a pair of inner and outer threaded portions, the airtight housing unit 40 can be installed in the pressurizing unit 30, and the periphery of the other end face side of the pressurizing unit 30 where the bolt member 32 (pressurizing mechanism) is exposed can be sealed.

[0136] Therefore, even for the assembly operation performed from the outside of the glove box while wearing gloves, the operator can easily perform this operation.

[0137] In these screwing operations, no special tools are required. For example, one of the units to be screwed can be fixed, and the other unit can be held, and the screwing operation can be easily performed manually.

[0138] In addition, in the present embodiment, as Figure 3 shown, on the outer peripheral surface of the battery housing unit 20 and the outer peripheral surface of the pressurizing unit 30, operating rods 52 for screwing operations are provided to protrude in the radial direction. The operator can more easily perform the above-mentioned screwing operations by simply turning the operating rod 52 by hand.

[0139] In addition, since the external threaded portion 23 is formed on the metal battery housing unit 20, as Figure 3 shown, the internal threaded portion 35 that is threadedly engaged with the external threaded portion 23 is formed on the inner peripheral surface of the metal ring 36, and a structure is formed in which the metal ring 36 is installed on the outer main body portion 30A of the synthetic resin pressurizing unit 30 using a fastener 50 such as a bolt. Thereby, the internal threaded portion 35 can have the same wear resistance, strength, etc. as the external threaded portion 23.

[0140] In addition, on one end face of the pressurizing unit 30 that is in close contact with one end face side of the battery housing unit 20, an O-ring 51 serving as a sealing member is provided. Further, on one end face of the airtight housing unit 40 that is in close contact with the other end face side of the pressurizing unit 30, an O-ring 51 serving as a sealing member is also provided. By introducing these O-rings 51, even with a screwing operation performed only by hand, it is possible to easily seal between the respective units.

[0141] Return Figure 1 , the battery analysis structure of the present embodiment is externally provided with a first electrode terminal 15 and a second electrode terminal 42.

[0142] The first electrode terminal 15 is fixed to the outer surface of the pressure receiving unit 10 by a fastener 50 such as a bolt. The pressure receiving unit 10 is formed of a conductive metal material. Thus, as Figure 2As shown, a state is formed in which the first electrode terminal 15 is electrically connected to one of the electrode active material layers of the test battery S via the pressure receiving unit 10 and the conductive partition member 12 (current collector layer).

[0143] The second electrode terminal 42 is fixed to the outer peripheral surface of the airtight housing unit 40 by a fastener 50 such as a bolt. Inside the airtight housing unit 40, a conductive member 43 electrically connected to the second electrode terminal 42 is arranged. The conductive member 43 is formed of a metal plate having spring characteristics, and when the airtight housing unit 40 is mounted on the pressurizing unit 30, the head of the bolt member 32 is positioned so as to abut against the conductive member 43.

[0144] Thus, as Figure 2 shown, the second electrode terminal 42 is in a state of being electrically connected to the other electrode active material layer of the test battery S through a conduction path formed by the conductive member 43, the bolt member 32, the pressure transmission member 33, the force measuring sensor 34, and the pressing member 22.

[0145] Therefore, by passing an electric current between the first electrode terminal 15 and the second electrode terminal 42, the test battery S accommodated inside the battery accommodation unit 20 can be charged, and in addition, by making these electrode terminals conduct through a resistor, the test battery S can be discharged.

[0146] As Figure 2 shown, the space between the first electrode terminal 15 and the second electrode terminal 42 is insulated by the synthetic resin outer main body portion 30A of the pressurizing unit 30 and the airtight housing portion 40 also made of synthetic resin.

[0147] As Figure 7A shown, the battery analysis structure according to the present embodiment with the above structure can be mounted on the specimen stage of an X-ray diffractometer, and X-ray diffraction measurement can be performed in the atmosphere. Here, a structure is formed such that by simply aligning and mounting a preset reference end face 44a with a reference face provided on the specimen stage of the X-ray diffractometer, the longitudinal direction of the X-ray window 11 can be positioned in the incident direction of the X-rays.

[0148] As Figure 7B shown, an arc-shaped long hole 45 is formed in the base 44, and the base 44 is fixed to the airtight housing unit 40 by passing a fastener 50 such as a bolt through the long hole 45. By loosening the fastener 50 and rotating the sealed housing unit 40 relative to the base 44 along the long hole 45, the orientation between the reference end face 44a of the base 44 and the X-ray window 11 can be adjusted in advance.

[0149] Next, referring to Figure 8, a method for analyzing and evaluating a test battery using the battery analysis structure according to the present embodiment will be described.

[0150] First, the block holder 13 is attached to the pressure receiving unit 10 (step S1). Then, the pressure receiving unit 10 is attached to the battery housing unit 20 (step S2). Further, the separator 12 (current collector layer), which is a separating member, is disposed on the back surface of the pressure receiving unit 10, and the insulating member 21 is attached to the battery housing unit 20 (step S3). Thus, the separator 12 (current collector layer) is pressed against the back surface of the pressure receiving unit 10, and the X-ray window 11 is sealed.

[0151] The operations up to this point can be performed outside the glove box.

[0152] Next, the necessary components, battery materials, pressure display, etc. are placed inside the glove box filled with an inert gas (e.g., argon) (step S4).

[0153] The operator wears the gloves equipped on the glove box and first forms the test battery S inside the glove box (step S5). Then, the formed test battery S is placed inside the battery housing unit 20, and the pressing member 22 is inserted into the battery housing unit 20 (step S6).

[0154] Next, the pressurizing unit 30 is attached to the battery housing unit 20 (step S7). Further, the pressure display is connected to the force sensor 34 (step S8).

[0155] After the operations up to this point are completed, while observing the pressure display, the bolt member 32 is screwed in to apply pressure to the test battery S inside the battery housing unit 20 (step S9). A tool such as a wrench is used to perform the screwing operation of the bolt member 32. And when the pressure applied to the test battery S reaches the target value, the screwing operation of the bolt member 32 is ended (step S10).

[0156] Next, the airtight housing unit 40 is attached to the pressurizing unit 30 (step S11), and the pressure display is removed from the force sensor 34 (step S12). By attaching the airtight housing unit 40, the assembly operation of the battery analysis structure is completed.

[0157] After that, the battery analysis structure is taken out of the glove box (step S13), and the block holder 13 is removed from the pressure receiving unit 10 (step S14).

[0158] Next, the battery analysis structure is installed in the X-ray diffractometer (step S15), and the charge / discharge device is connected to the first and second electrode terminals 15 and 42 (step S16). Then, while charging and discharging the test battery S, X-ray diffraction measurement is performed on the test battery S (step S17), and the characteristics of the test battery S are analyzed and evaluated using the measurement data. Here, during or after the X-ray diffraction measurement, a pressure display can be connected to the output rod 34a to measure the pressure acting on the test battery S. Thus, the measurement results obtained by X-ray diffraction measurement can be analyzed and evaluated in relation to the pressure of the test battery S.

[0159] In addition, after charging and discharging the test battery S, X-ray diffraction measurement can be performed on the test battery S.

[0160] Figure 9 It is a graph showing the results of observing the state changes (phase state changes caused by the insertion and extraction of lithium ions) during the charge and discharge process of the negative electrode active material for all-solid-state batteries using the battery analysis structure according to the present embodiment with an X-ray diffractometer. A pressure of 9.8 MPa is applied to the test battery.

[0161] As shown in this graph, the state changes of each phase generated during charge and discharge can be clearly observed from the changes in the peaks of the diffracted X-rays.

[0162] 〔Second Embodiment〕

[0163] Next, with reference to Figures 10 to 17 , the battery analysis structure according to the second embodiment of the present invention will be described in detail.

[0164] In addition, in the battery analysis structure according to the second embodiment of the present invention, the same reference numerals are given to the same or corresponding parts as those in the battery analysis structure according to the first embodiment of the present invention shown in Figures 1 to 8 , and the detailed description thereof is omitted.

[0165] Figure 10 It is a perspective view showing the appearance of the battery analysis structure according to the present embodiment, Figure 11 and it is an exploded front cross-sectional view of the battery analysis structure. Figure 10 Corresponding to Figure 1 , in addition, Figure 11 Corresponding to Figure 4 .

[0166] In the first embodiment described above, for example, as in Figure 1 and Figure 4As shown, the pressure receiving unit 10 and the battery housing unit 20 are respectively configured to be composed of separate units, and the pressure receiving unit 10 is press-fitted and fixed to the battery housing unit 20 by the fastener 50.

[0167] In contrast, in the present embodiment, the pressure receiving unit 10 and the battery housing unit 20 are integrally formed and constituted by a single pressure receiving and battery housing unit 100.

[0168] That is, the pressure receiving and battery housing unit 100 is a unit including the pressure receiving unit 10 and the battery housing unit 20 in the first embodiment described above, and has the functions of the respective units 10 and 20 as they are.

[0169] In addition, except for the content regarding the installation of the pressure receiving unit 10 to the battery housing unit 20 using the fastener 50, the descriptions of the pressure receiving unit 10 and the battery housing unit 20 in the first embodiment also apply to the pressure receiving and battery housing unit 100 as they are.

[0170] In addition, in the present embodiment, in the first embodiment described above, the flat base 44 installed on the lower end face side of the airtight housing unit 40 is omitted, and the lower part of the airtight housing unit 40 is configured to be installed on the base 101 of the X-ray diffractometer to be described later. The base 101 includes a circular bottom surface 101a formed in the airtight housing unit 40 and a circumferential surface 101b (only the lower region) erected from the bottom surface 101a (see Figure 11 ).

[0171] The X-ray diffractometer to which the battery analysis structure according to the present embodiment is installed is equipped with an Figure 12 installation table 200 as shown. The battery analysis structure is rotatably installed on the installation table 200.

[0172] A circumferential groove 201 for arranging the battery analysis structure is formed in the installation table 200. And, as Figures 13 to 14 shown, by arranging the base 101 of the airtight housing unit 40 in the battery analysis structure 1 in the circumferential groove 201, the battery analysis structure 1 is supported on the bottom surface of the circumferential groove 201 and installed on the installation table 200. Furthermore, the battery analysis structure 1 can be guided by the inner circumferential surface of the circumferential groove 201 and rotate freely.

[0173] In addition, on the installation table 200, a positioning block 202 is erected outside the circumferential groove 201, and a positioning portion 202a is formed on a partial inner side surface of the positioning block 202 (see Figure 14 ).

[0174] On the other hand, in the battery analysis structure 1, an operation lever 52 is provided so as to project radially from the outer peripheral surface of the pressure-receiving / battery housing unit 100 (the battery housing unit 20 in the first embodiment), and this operation lever 52 also functions as a positioning abutting portion. That is, as Figure 14 shown, the battery analysis structure 1 mounted on the mounting table 200 is rotated, and as Figure 15 shown, the positioning abutting portion 52 is brought into contact with the positioning portion 202a, whereby the X-ray window 11 of the battery analysis structure 1 can be positioned with respect to the X-ray a irradiated from the X-ray diffractometer.

[0175] Here, in a state where the positioning abutting portion 52 is in contact with the positioning portion 202a, the positional relationship between the positioning portion 202a and the positioning abutting portion 52 and the positional relationship between the positioning abutting portion 52 and the X-ray window 11 are adjusted in advance so that the central trajectory of the X-ray a irradiated from the X-ray source of the X-ray diffractometer is arranged in the same vertical plane as the length direction of the opening of the long-hole-shaped X-ray window 11, and the X-ray a is incident from the X-ray window 11 and irradiated onto the internal specimen battery S.

[0176] In addition, the positioning abutting portions 52 are provided so as to project from two positions that are symmetric with respect to the rotation center when rotating on the mounting table 200, and by selecting any one of them to be in contact with the positioning portion 202a, the X-ray a can be incident from a direction that is 180 degrees different from the X-ray window 11 (refer to Figure 15 ).

[0177] In addition, as Figure 16 shown, the slit device 203 can be detachably mounted on the positioning block 202 provided on the mounting table 200. The slit device 203 can be, for example, a slit device called a Schulz slit, whereby the width of the X-ray a irradiated from the X-ray source to the X-ray window 11 is restricted. Thus, since scattering generated by the X-ray irradiating outside the specimen battery S can be reduced, highly accurate X-ray diffraction measurement can be achieved.

[0178] Figure 17 is a perspective view showing the appearance of the X-ray diffractometer on which the battery analysis structure is mounted.

[0179] As shown in this figure, the battery analysis structure 1 is mounted on the mounting table 200 of the X-ray diffractometer. The X-ray a irradiated from the X-ray source 210 is incident on the X-ray window 11 via the slit device 203. And the X-ray detector 220 detects the diffracted X-ray b reflected from the specimen battery S accommodated inside the battery analysis structure 1, whereby X-ray diffraction measurement of the specimen battery S can be performed.

[0180] 〔Modification Example or Application Example〕

[0181] In addition, it goes without saying that the present invention is not limited to the above-described embodiments, but various modifications or applications can be made.

[0182] For example, for the battery analysis structure of the present invention, the sample battery to be analyzed is not limited to all-solid-state batteries, and can also be applied to the analysis and evaluation of various other batteries such as lithium-ion batteries.

[0183] In addition, for the assembly of the battery analysis structure according to the present invention, a glove box is not essential, and depending on the type of the sample battery, an assembly without using a glove box can also be used.

[0184] The structures of each component such as the pressure-bearing unit, the battery accommodation unit, the pressurizing unit, the airtight housing unit, and the insulating member are not limited to the structures of the above-described embodiments. For example, any part of each component is made of a material having conductivity or insulation. However, depending on the installation position of each electrode terminal, etc., appropriate design changes can also be made.

[0185] In addition, as Figure 18 shown, a recess 61 may be provided in the peripheral area on the back surface of the X-ray window 11 formed in the pressure-bearing unit 10, and a window embedding member 60 formed of thin-plate glassy carbon (glass carbon) or beryllium may be disposed in the recess 61. The window embedding member 60 is attached to the back surface of the pressure-bearing unit 10 by an adhesive or by brazing.

[0186] The back surface of the window embedding member 60 is disposed on the same plane as the surface 10a on which the partition member 12 is disposed on the back surface of the pressure-bearing unit 10.

[0187] Glassy carbon or beryllium has the property of transmitting X-rays and isolating the atmosphere. Moreover, due to its high pressure resistance, even when the pressure acting on the sample battery S is applied, it will not be pressed into the cutout hole of the X-ray window 11, and can support the partition member 12 (current collector layer) and the sample battery S with a flat surface.

[0188] The structure of the base 101 in the airtight housing unit 40 shown in the second embodiment, the structure of the mounting table 200 of the X-ray diffractometer (refer to Figure 12 ), the positioning structure of the X-ray window 11 formed by the positioning portion 202a and the positioning abutting portion (operation portion 52) (refer to Figure 15 ), the setting structure of the slit device 203, etc. can also be applied to the battery analysis structure according to the first embodiment.

Claims

1. A structure for battery analysis, characterized in that, Equipped with: A specimen battery, the structure of the specimen battery being: electrode active material layers are arranged on both end sides of an electrolyte layer, and further, current collector layers are respectively arranged outside each electrode active material layer; A battery housing unit, the battery housing unit being formed with a hollow portion for housing the specimen battery; A pressurizing unit, the pressurizing unit being installed on one end face side of the battery housing unit, and being equipped with a pressurizing mechanism for applying pressure to the specimen battery housed in the hollow portion of the battery housing unit; And A pressure receiving unit, the pressure receiving unit being fixed to the other end face side of the battery housing unit, and receiving the pressure acting on the specimen battery, In the pressure receiving unit, an X-ray window is formed by a cutout hole penetrating from the front surface to the back surface, the X-ray window being used for irradiating the specimen battery housed in the hollow portion of the battery housing unit with X-rays, and for emitting diffracted X-rays reflected from the specimen battery to the outside, In the X-ray window, a partitioning member is arranged, the partitioning member allowing X-rays to pass through, but isolating the hollow portion inside the battery housing unit from the atmosphere.

2. The battery analysis structure according to claim 1, wherein The pressure receiving unit and the battery housing unit are integrally formed.

3. The battery analysis structure according to claim 1, wherein The X-ray window is formed with a smaller width compared to the pressing region where the specimen battery housed in the hollow portion of the battery housing unit abuts against the partitioning member.

4. The battery analysis structure according to claim 1, wherein The pressurizing mechanism at least has a bolt member for adjusting the pressure acting on the specimen battery, In the pressurizing unit, a nut portion that is threadedly engaged with the bolt member is formed, In the hollow portion of the battery housing unit, a pressing member is inserted, and the specimen battery receives the pressure from the bolt member via the pressing member.

5. The battery analysis structure according to claim 1, characterized in that, An insulating member is equipped, the insulating member being embedded in the hollow portion of the battery housing unit, insulating the outer peripheral surface of the specimen battery housed in the hollow portion, and closing the X-ray window, The front end face of the insulating member is pressed against the partitioning member via an airtight member, and the partitioning member is in close contact with the periphery of the X-ray window by the pressing force to close the X-ray window.

6. The structure for battery analysis according to claim 5, characterized in that, Internal and external thread portions are provided between one end face side of the battery housing unit and one end face side of the pressurizing unit installed on the one end face side, and the one end face side of the pressurizing unit is installed on the one end face side of the battery housing unit by screwing operation of the thread portions to seal between the units.

7. The battery analysis structure according to claim 6, wherein For the pressurizing unit, the pressurizing mechanism is exposed on the other end face side where the thread portions are not provided, and an airtight housing unit is equipped, the airtight housing unit hermetically sealing the periphery of the pressurizing mechanism exposed on the other end face side of the pressurizing unit. Internal and external second thread portions are provided between the other end face side of the pressurizing unit and one end face side of the airtight housing unit installed on the other end face side, and the one end face side of the airtight housing unit is installed on the other end face side of the pressurizing unit and sealed by screwing operation of the second thread portions.

8. The battery analysis structure according to claim 1, wherein A first electrode terminal and a second electrode terminal are provided on the outside. The first electrode terminal is electrically connected to one of the current collector layers, and the second electrode terminal is electrically connected to the other current collector layer.

9. The battery analysis structure according to claim 8, wherein the first electrode terminal is provided outside the pressure receiving unit, the pressure receiving unit is composed of a conductive metal component, and one of the current collector layers is electrically connected to the first electrode terminal via the pressure receiving unit.

10. The battery analysis structure according to claim 8, characterized in that, The pressing mechanism is composed of a conductive metal component, and the other current collector layer is electrically connected to the second electrode terminal via the pressing mechanism.

11. The structure for battery analysis according to claim 8, characterized in that, The separating member is configured as one of the current collector layers constituting the sample battery, The pressing mechanism presses the sample battery and the separating member against the back surface of the pressure receiving unit so that the separating member is in close contact with one of the electrode active material layers constituting the sample battery.

12. The battery analysis structure according to claim 1, wherein A block holder is provided, which is configured to be inserted from the front opening of the X-ray window, and the front end surface is buried in the back opening of the X-ray window.

13. The battery analysis structure according to claim 4, wherein The pressing unit is provided with an output unit that outputs an electrical signal related to the pressure acting on the pressing member.

14. The battery analysis structure according to claim 1, wherein A recess is provided in the periphery of the back surface of the X-ray window formed in the pressure receiving unit, and a thin plate-shaped glassy carbon or beryllium is disposed in the recess.

15. The battery analysis structure according to claim 1, which is rotatably mounted on an X-ray diffractometer, wherein a positioning abutting portion is provided, which abuts against a positioning portion provided on the X-ray diffractometer to position the X-ray window with respect to the X-ray irradiated from the X-ray diffractometer.

16. The battery analysis structure according to claim 15, characterized in that, The positioning abutting portions are provided at two positions that are symmetric with respect to the rotation center when rotating rotatably with respect to the X-ray diffractometer.

17. The battery analysis structure according to claim 1, which is rotatably mounted on an X-ray diffractometer, wherein a base is provided, which is disposed on a mounting table formed by a circular groove provided in the X-ray diffractometer, has a circular bottom surface and a circumferential surface, and is guided by the circular groove of the mounting table to rotate freely.

18. An X-ray diffraction device, characterized in that, The battery analysis structure according to any one of claims 1 to 17 is mounted, and X-rays are irradiated through the X-ray window onto a sample battery accommodated in the hollow portion of the battery accommodation unit, thereby performing X-ray diffraction measurement.

19. The X-ray diffraction apparatus according to claim 18, characterized in that, It has: a positioning block having a positioning portion for positioning the X-ray window of the battery analysis structure; and a slit device that is detachable with respect to the positioning block and is used to reduce X-ray scattering generated from sources other than the sample battery accommodated in the hollow portion of the battery accommodation unit.

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